Abstract.A series of vanadia-titania (V-Ti) xerogel catalysts were prepared by nonhydrolytic sol-gel method. These catalysts showed much higher surface area and total pore volumes than the conventional V2O5-TiO2 xerogel. Two species of surface vanadium in the xerogel catalysts were identified by Raman measurements: monomeric vanadyl and polymeric vanadates. The selective oxidation of hydrogen sulfide in the presence of excess water and ammonia was studied over these catalysts. Xerogel catalysts from the nonhydrolytic method showed very high conversion of H2S without harmful emission of SO2. The conversion of H2S increased with increasing vanadia loading up to 10V-Ti; however, it decreased at higher vanadia loading (12V-Ti and 18V-Ti) probably due to the formation of crystalline V2O5.